تفاعل #1687624

معادلة التفاعل

hydrochloric acid

sodium carbonate

thiosemicarbazide

nicotinoyl chloride

→

3-Mercapto-5(3-pyridyl)-1,2,4-triazole

المذيبات

water

pyridine

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter reflux for 40 min. the reaction mixture
2. 2
   تركيزwas concentrated to half the original volume, 500 ml of water
3. 3
   workup.ADDITIONwas added
4. 4
   أخرىstored in the cold overnight
5. 5
   أخرىformed
6. 6
   أخرىwas removed by filtration
7. 7
   أخرىthe filtrate was evaporated in vacuo
8. 8
   workup.DISSOLUTIONThe resulting heavy, yellow oil was dissolved in 300 ml of water
9. 9
   درجة الحرارةAfter reflux for 4 h the solution
10. 10
    درجة الحرارةwas cooled
11. 11
    أخرىThe formed, colorless precipitate, 65, was isolated by filtration
12. 12
    أخرىdried in vacuo

الإجراء التجريبي

To a solution of 19 g (0.200 mol) of thiosemicarbazide in 175 ml of dry pyridine, 29 g (0.200 mol) of nicotinoyl chloride was slowly added at 10° C. After reflux for 40 min. the reaction mixture was concentrated to half the original volume, 500 ml of water was added, and stored in the cold overnight The precipitate formed was removed by filtration, and the filtrate was evaporated in vacuo. The resulting heavy, yellow oil was dissolved in 300 ml of water, and 64 g (0.600 mol) of sodium carbonate in 400 ml of water was added. After reflux for 4 h the solution was cooled and acidified with conc. hydrochloric acid to pH=4. The formed, colorless precipitate, 65, was isolated by filtration and dried in vacuo. Yield: 35 g (0.297 mol, 98%).

المصدر